WO2016080459A1 - 焼結体 - Google Patents

焼結体 Download PDF

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Publication number
WO2016080459A1
WO2016080459A1 PCT/JP2015/082452 JP2015082452W WO2016080459A1 WO 2016080459 A1 WO2016080459 A1 WO 2016080459A1 JP 2015082452 W JP2015082452 W JP 2015082452W WO 2016080459 A1 WO2016080459 A1 WO 2016080459A1
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WIPO (PCT)
Prior art keywords
sintered body
mpa
yttrium oxyfluoride
yttrium
sintering
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PCT/JP2015/082452
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English (en)
French (fr)
Japanese (ja)
Inventor
豊彦 矢野
克己 吉田
徹 津之浦
勇二 重吉
Original Assignee
日本イットリウム株式会社
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Application filed by 日本イットリウム株式会社 filed Critical 日本イットリウム株式会社
Priority to US15/510,136 priority Critical patent/US9969652B2/en
Priority to KR1020177007138A priority patent/KR101823493B1/ko
Priority to CN201580050549.4A priority patent/CN107074663B/zh
Publication of WO2016080459A1 publication Critical patent/WO2016080459A1/ja

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Definitions

  • the present invention relates to a sintered body containing an yttrium oxyfluoride.
  • Fluorine-based corrosive gas, chlorine-based corrosive gas, and plasma using these are used in each process of semiconductor manufacturing, particularly dry etching, plasma etching, and cleaning. These corrosive gases and plasma corrode the constituent members of the semiconductor manufacturing apparatus, and fine particles separated from the surface of the constituent members tend to adhere to the semiconductor surface and cause product defects. Therefore, ceramics having high corrosion resistance against halogen-based plasma must be used as a bulk material for constituent members of a semiconductor manufacturing apparatus.
  • aluminum oxide, yttrium oxide, aluminum yttrium composite oxide, and yttrium fluoride are used as such bulk materials (see Patent Documents 1 to 3).
  • Patent Document 4 The applicant has previously proposed a thermal spray material containing yttrium oxyfluoride as a corrosion resistant material used to prevent corrosion of the etching apparatus.
  • Aluminum-containing compounds such as aluminum oxide are concerned about aluminum contamination of semiconductor silicon. It has been pointed out that the plasma resistance of yttrium oxide is insufficient, and the surface is altered and yttrium fluoride (YF 3 ) is formed by fluorine plasma irradiation. Since yttrium fluoride is a fluoride, its chemical stability is questionable. In addition, when the inside of a semiconductor device is coated using yttrium oxyfluoride as a thermal spray material, there is a limit to the denseness of the resulting coating film, and it cannot be said that the performance of blocking halogen-based corrosive gas is sufficient. .
  • an object of the present invention is to provide a sintered body that can eliminate various drawbacks of the above-described conventional technology.
  • the present invention provides a sintered body containing yttrium oxyfluoride.
  • the present invention is a method for producing the sintered body, Obtaining a raw material powder compact containing yttrium oxyfluoride; And obtaining the sintered body by sintering the molded body at a temperature of 800 ° C. or higher and 1800 ° C. or lower under a pressure of 5 MPa or higher and 100 MPa or lower. is there.
  • the present invention is a method for producing the sintered body, Obtaining a raw material powder compact containing yttrium oxyfluoride; And a step of sintering the molded body at a temperature of 1000 ° C. or more and 2000 ° C. or less under no pressure.
  • the sintered body of the present invention exhibits excellent resistance to halogen-based plasma, and is useful as a constituent material for semiconductor manufacturing apparatuses such as etching apparatuses. Moreover, the manufacturing method of the sintered compact of this invention can manufacture a dense sintered compact efficiently as a sintered compact of this invention.
  • FIG. 2 is an X-ray chart by powder XRD diffraction measurement of the sintered body obtained in Example 1.
  • FIG. 4 is an X-ray chart by powder XRD diffraction measurement of the sintered body obtained in Example 2.
  • FIG. 6 is an X-ray chart by powder XRD diffraction measurement of the sintered body obtained in Example 3.
  • FIG. 6 is an X-ray chart by powder XRD diffraction measurement of the sintered body obtained in Example 4.
  • FIG. 3 is a SEM photograph of the sintered body obtained in Example 2 before and after plasma irradiation. It is a SEM photograph before and after plasma irradiation of the single crystal silicon which is the comparative example 1.
  • FIG. 3 is a SEM photograph of the sintered body obtained in Example 2 before and after plasma irradiation. It is a SEM photograph before and after plasma irradiation of the single crystal silicon which is the comparative example 1.
  • FIG. 3 is a SEM photograph of the sintered body
  • FIG. It is a SEM photograph before and after plasma irradiation of the alumina which is the comparative example 2.
  • FIG. It is a SEM photograph before and after plasma irradiation of the yttria which is the comparative example 3.
  • FIG. It is a SEM photograph before and behind plasma irradiation of the yttrium fluoride which is the comparative example 4.
  • FIG. It is a graph which shows the change of F / O ratio before and behind plasma irradiation in the sample surface of an Example and a comparative example.
  • the sintered body of the present invention is characterized by containing yttrium oxyfluoride.
  • the yttrium oxyfluoride in the present invention is a compound composed of yttrium (Y), oxygen (O), and fluorine (F).
  • Examples of such compounds include Y 5 O 4 F 7 and Y 7 O 6 F 9 , and among these, one or more oxyfluorides are included. These can be used alone or in combination of two or more.
  • YOF a sintered body excellent in mechanical strength can be obtained, a dense sintered body having no cracks can be obtained, and it has advantages such as excellent corrosion resistance compared to other compositions.
  • Y 5 O 4 F 7 a dense sintered body without cracks can be obtained at a low temperature, and the formation of YOF after oxidation improves the corrosion resistance.
  • the present invention by using yttrium oxyfluoride as a sintered body instead of a thermal spray material, it is possible to improve the barrier property of halogen-based corrosive gas.
  • a thermal spray material When a thermal spray material is used, the particles formed from the thermal spray material are melted by thermal spraying to form a thermal spray film, and halogen-based corrosive gas flows into the minute gaps between the melted particles. There is.
  • the sintered body has high density and excellent barrier properties against halogen-based corrosive gas. Therefore, when this is used as a component of a semiconductor device, for example, the flow of halogen-based corrosive gas into this member is prevented. Can be prevented.
  • the sintered body of the present invention has a high performance of preventing corrosion caused by halogen-based corrosive gas.
  • a member having a high barrier property against halogen-based corrosive gas is suitably used for, for example, a vacuum chamber constituent member of an etching apparatus, an etching gas supply port, a focus ring, a wafer holder and the like.
  • the sintered body preferably has a relative density of 70% or more, more preferably 80% or more, and 90% or more. More preferred is 95% or more.
  • the relative density (RD) is preferably as high as possible, and the upper limit is 100%.
  • the porosity is preferably small.
  • the open porosity is determined by the method described below, preferably 10% or less, more preferably 2% or less, and particularly preferably 0.5% or less.
  • RD relative density
  • OP open porosity
  • the relative density (RD) and the open porosity can be measured by Archimedes method based on JIS R1634, and specifically by the following method.
  • ⁇ 1 [g / cm 3 ] is the density of distilled water.
  • the three-point bending strength ⁇ f of the sintered body of the present invention is a high value above a certain level.
  • the three-point bending strength ⁇ f of the sintered body of the present invention is preferably 10 MPa or more, more preferably 20 MPa or more, still more preferably 50 MPa or more, and 100 MPa or more. It is particularly preferred.
  • the higher the three-point bending strength ⁇ f the higher the strength as a constituent material of the semiconductor manufacturing apparatus, which is preferable.
  • the upper limit is 300 MPa or less, such as the ease of manufacturing the sintered body. It is preferable from the viewpoint.
  • the sintered body having the above strength can be obtained by producing the sintered body of the present invention by the production method (1) or (2) described later.
  • the three-point bending strength ⁇ f is measured by the following method.
  • ⁇ Method for measuring three-point bending strength ⁇ f > By cutting the sintered body and mirror polishing one side, a strip-shaped test piece having a thickness of 1.5 to 3.0 mm, a width of about 4 mm, and a length of about 35 mm is produced. This is placed on a SiC jig and a three-point bending test is performed with a universal material testing machine (1185 type, manufactured by INSTRON). The conditions are a distance between fulcrums of 30 mm, a crosshead speed of 0.5 mm / min, and the number of test pieces is 5. Based on JIS R1601, the bending strength ⁇ f [MPa] is calculated using the following equation.
  • ⁇ f (3 ⁇ P f ⁇ L) / (2 ⁇ w ⁇ t 2 ) (MPa)
  • P f is the load [N] when the test piece is broken
  • L is the span distance [mm]
  • w is the width [mm] of the test piece
  • t is the thickness [mm] of the test piece.
  • the sintered body of the present invention preferably has an elastic modulus of 25 GPa or more and 300 GPa or less, more preferably 50 GPa or more and 300 GPa or less, more preferably 100 GPa or more and 250 GPa or less, and most preferably 150 GPa or more and 200 GPa or less. is there.
  • an elastic modulus of 25 GPa or more and 300 GPa or less, more preferably 50 GPa or more and 300 GPa or less, more preferably 100 GPa or more and 250 GPa or less, and most preferably 150 GPa or more and 200 GPa or less. is there.
  • the elastic modulus By setting the elastic modulus in such a range, the material constituting the semiconductor manufacturing apparatus has high durability and exhibits excellent resistance to halogen-based plasma.
  • One method for obtaining such an elastic modulus is a method of adjusting the average particle diameter of the raw material powder, the forming method, the pressing method, etc. in the method for producing a sintered body described
  • the elastic modulus is obtained by the following method according to JIS R1602.
  • the measurement uses an oscilloscope (WJ312A, manufactured by LECROY) and a pulsar receiver (5072PR, manufactured by Olympus NDT).
  • Longitudinal wave vibrator (V110, 5 MHz) and transverse wave vibrator (V156, 5 MHz) are used for the test piece. ))
  • the longitudinal wave velocity V l [m / s] and the transverse wave velocity V t [m / s] are measured from the propagation velocity of the pulse.
  • the sintered body of the present invention preferably has a thermal conductivity of 5.0 W / (m ⁇ K) or more, more preferably 10.0 W / (m ⁇ K) or more.
  • the sintered body having a high thermal conductivity can be suitably used for a component member that requires uniform temperature and a component member having a large temperature change.
  • the thermal conductivity of the sintered body is 5.0 W / (m It is also preferable that the value is as low as K) or less, particularly about 3.0 W / (m ⁇ K) or less.
  • the thermal conductivity can be measured as follows.
  • ⁇ Measurement method of thermal conductivity> A square plate sample having a side of 10 mm and a thickness of 1 mm was used. Platinum coating was applied to both surfaces of the sample, and a spray containing carbon particles (FC-153, manufactured by Fine Chemical Japan) was thinly sprayed thereon. The blackened sample was placed in a jig, the surface was irradiated with a pulse (pulse width 0.33 ms) by a xenon flash lamp, and the temperature change on the back surface of the sample was measured to obtain the thermal diffusivity ⁇ . The temperature change was 10 times the half time as the calculation range. In addition, specific heat capacity C was determined using alumina as a standard sample.
  • the sintered body of the present invention may be substantially composed only of yttrium oxyfluoride, but may contain components other than yttrium oxyfluoride. “Substantially” means that only unavoidable impurities are contained in addition to oxyfluoride, and specifically means that the content of oxyfluoride is 98% by mass or more. Examples of the inevitable impurities herein include by-products such as yttrium oxide produced by the following method (1) or (2).
  • the content of the yttrium oxyfluoride in the sintered body of the present invention is 50% by mass or more from the viewpoint of further enhancing the plasma resistance effect of the present invention, and the mechanical strength. It is preferable from the viewpoint of improvement. From this viewpoint, the amount of yttrium oxyfluoride in the sintered body is more preferably 80% by mass or more, further preferably 90% by mass or more, and particularly preferably 98% by mass or more. The higher the yttrium oxyfluoride content in the sintered body, the better.
  • the content of yttrium oxyfluoride in the sintered body can be measured by the following method.
  • the qualitative analysis in this case can be performed by, for example, X-ray diffraction measurement. X-ray diffraction measurement is performed on a powder sample in which yttrium oxide and yttrium oxyfluoride are mixed at a certain ratio. Of the obtained diffraction peaks, the ratio of the maximum peak intensity of yttrium oxide and the maximum peak intensity of yttrium oxyfluoride is taken and plotted against the mixing ratio to create a calibration curve.
  • the mixing ratio of yttrium oxide and yttrium oxyfluoride is measured, and the ratio of yttrium oxyfluoride when the sum of the two is 100 is taken as the content of yttrium oxyfluoride.
  • the X-ray diffraction measurement of the sintered body is a measurement of the sintered body as a powder, and can be performed by the method described in the examples described later.
  • the substance and the oxyfluoride are analyzed in the same manner as described above. What is necessary is just to obtain
  • the maximum peak height derived from yttrium oxyfluoride in the above scanning range is 1, the maximum peak height derived from components other than yttrium oxyfluoride is preferably 0.5 or less. , 0.05 or less is more preferable.
  • the maximum peak height derived from YF 3 is 0. 1 or less is preferable, and 0.03 or less is more preferable.
  • the maximum peak height derived from Y 2 O 3 is 0.2.
  • X-ray diffraction measurement of the sintered powder can be performed by the method described in the examples described later.
  • the peak ratio in the sintered body of the present invention can be set in the above range by adjusting the ratio of yttrium oxyfluoride in the raw material powder, the temperature of the sintering conditions, the sintering atmosphere, and the like.
  • the sintered body of the present invention comprises a YOF, preferably contains rhombohedral as the YOF, if the sintered body of the present invention comprises a Y 5 O 4 F 7, oblique as the Y 5 O 4 F 7 It is preferable to include a tetragonal crystal. These crystal phases can be identified by performing X-ray diffraction measurement of the sintered body surface or powder.
  • examples of components other than yttrium oxyfluoride include various sintering aids, binder resins, carbon, and the like.
  • the sintered body of the present invention includes conventionally used aluminum oxide, yttrium oxide, aluminum yttrium composite oxide, yttrium fluoride, and other rare earth element-containing compounds other than yttrium.
  • Various ceramic materials such as these may be contained.
  • the sintered body of the present invention is a sintered body containing yttrium oxyfluoride, it has excellent resistance to halogen-based plasma as compared with sintered bodies of other ceramic materials. Compared with the thermal spray material containing yttrium oxyfluoride, it is excellent in denseness and barrier property against halogen-based corrosive gas.
  • Examples of the method for producing a sintered body of the present invention include the following method (1). (1) a step of obtaining a molded body of raw material powder containing yttrium oxyfluoride; A step of obtaining the sintered body by sintering the molded body at a temperature of 800 ° C. to 1800 ° C. under a pressure of 5 MPa to 100 MPa.
  • the step of obtaining a molded body and the step of sintering the molded body may be performed simultaneously.
  • the method (1) includes putting a powder sample into a mold and pressure-sintering the powder sample as it is.
  • Examples of the yttrium oxyfluoride in the raw material powder containing the yttrium oxyfluoride include those similar to the yttrium oxyfluoride contained in the sintered body.
  • the yttrium oxyfluoride used as a raw material is usually in powder form.
  • the average particle diameter of the yttrium oxyfluoride contained in the raw material powder is preferably 5 ⁇ m or less, more preferably 1.5 ⁇ m or less, still more preferably 1.1 ⁇ m or less, and particularly preferably 1 ⁇ m or less. preferable.
  • the average particle diameter is a 50% diameter (hereinafter also simply referred to as “D50”) in the volume-based integrated fraction, and is measured by a laser diffraction / scattering particle size distribution measurement method.
  • the specific measurement method is as follows.
  • As a preferable particle diameter of the average particle diameter of the raw material powder the same particle diameter as the average particle diameter of the yttrium oxyfluoride contained in the raw material powder can be mentioned.
  • Measurement method of average particle size Measure with Microtrack HRA manufactured by Nikkiso Co., Ltd. At the time of measurement, a 2 mass% sodium hexametaphosphate aqueous solution is used as a dispersion medium, and the sample (granule) is added to the sample circulator chamber of Microtrac HRA until the apparatus determines that the concentration is appropriate.
  • the above-mentioned sintering aids and binders may be used as the other components in the raw material powder.
  • the sintered body of the present invention includes sintering aids and binder resins.
  • the amount of other components is preferably small.
  • the sintering aid is preferably 5% by mass or less, and more preferably 2% by mass or less.
  • the production method of the present invention is characterized in that a dense sintered body can be obtained even if a sintering aid is not used or the amount thereof is reduced as much as possible.
  • the sintering aid here include SiO 2 , MgO, CaO, and various rare earth oxides.
  • a die press method for molding the raw material powder, a die press method, a rubber press (hydrostatic pressure press) method, a sheet molding method, an extrusion molding method, a casting molding method, or the like can be used.
  • the uniaxial pressure is preferably 20 MPa or more and 85 MPa or less, and more preferably 22 MPa or more and 75 MPa or less.
  • the pressure in the hydrostatic press is preferably 85 MPa or more and 250 MPa or less, and more preferably 100 MPa or more and 220 MPa or less.
  • the uniaxial pressure is preferably 10 MPa or more and 100 MPa or less, and more preferably 15 MPa or more and 80 MPa or less.
  • the content of yttrium oxyfluoride is preferably 80% by mass or more, more preferably 95% by mass or more, and particularly preferably 98% by mass or more.
  • the molded body obtained above is pressure-sintered.
  • a specific pressure sintering method hot pressing, pulse current pressing (SPS), hot isostatic pressing (HIP) can be used.
  • the pressure applied in the pressure sintering is preferably 5 MPa or more and 100 MPa or less. By setting the pressure to 5 MPa or more, a dense sintered body having high plasma resistance can be easily obtained, and by setting the pressure to 100 MPa or less, there are advantages such as suppressing damage to the press die. From these viewpoints, the pressure of pressure sintering is preferably 20 MPa or more, and more preferably 100 MPa or less.
  • the sintering temperature is preferably 800 ° C. or higher and 1800 ° C. or lower.
  • the temperature is 800 ° C. or higher, densification easily proceeds, decomposition and evaporation of the added binder proceeds, and unreacted components contained in the raw material react to form oxyfluoride.
  • the sintering temperature is more preferably 1000 ° C. or higher and 1700 ° C. or lower.
  • the time for pressure sintering at the pressure and temperature in the above range is preferably 0 hour or longer and 6 hours or shorter, and more preferably 20 minutes or longer and 2 hours or shorter.
  • the pressure for pressure sintering is preferably from 30 MPa to 50 MPa, and the sintering temperature is preferably from 1300 ° C. to 1700 ° C.
  • the pressure for pressure sintering is preferably 30 MPa or more and 100 MPa or less, and the sintering temperature is more preferably 1000 ° C. or more and 1500 ° C. or less.
  • the sintered body of the present invention can be preferably produced by the following method (2) instead of the method (1).
  • (2) a step of obtaining a molded body of raw material powder containing yttrium oxyfluoride; Sintering the molded body at a temperature of 1000 ° C. or more and 2000 ° C. or less under no pressure, and a method for producing a sintered body.
  • the method (2) differs from the method (1) in that pressureless sintering is performed, but the step of obtaining a raw material powder compact is the same as the method (1).
  • the sintering temperature is preferably 1000 ° C. or higher from the viewpoint of obtaining a dense sintered body and from the viewpoint of removing mixed organic substances, and the pressure of 2000 ° C. or lower is a pressure sintering apparatus that suppresses decomposition of oxyfluoride. It is preferable from the viewpoint of suppressing damage. From these viewpoints, the sintering temperature is more preferably 1200 ° C. or higher and 1800 ° C. or lower.
  • the time for sintering at the above sintering temperature is preferably 0 hour or longer and 24 hours or shorter, more preferably 0 hour or longer and 6 hours or shorter.
  • a sufficiently dense sintered body can be obtained by sintering the raw material powder at the above temperature even without pressureless sintering.
  • Sintering in any of the methods (1) and (2) may be performed in an oxygen-containing atmosphere or in an inert atmosphere. However, it is preferably performed in an inert atmosphere from the viewpoint of preventing the formation of yttrium oxide.
  • the oxygen-containing atmosphere includes air
  • the inert atmosphere includes a rare gas such as argon, nitrogen, and vacuum.
  • the sintering in any of the methods (1) and (2) is preferably performed at a temperature up to 1200 ° C. and at a temperature lowering of 0.5 ° C./min to 40 ° C./min. It is preferable to perform the temperature increase and decrease in the region at 1 ° C./min or more and 30 ° C./min or less.
  • the sintered body obtained in this manner can be used for constituent members of a semiconductor manufacturing apparatus such as a vacuum chamber in an etching apparatus and a sample stage, chuck, focus ring, and etching gas supply port in the chamber.
  • a semiconductor manufacturing apparatus such as a vacuum chamber in an etching apparatus and a sample stage, chuck, focus ring, and etching gas supply port in the chamber.
  • the sintered compact of this invention can be used for the use of various plasma processing apparatuses and the structural member of a chemical plant besides the structural member of a semiconductor manufacturing apparatus.
  • Example 1 (Production of sintered body containing YOF by pressureless sintering) About 1.4 g of YOF powder (average particle diameter 0.8 ⁇ m) was put in a circular mold having a diameter of 15 mm, and uniaxially pressed with a hydraulic press at a pressure of 25.5 MPa for 1 minute, followed by primary molding. The obtained primary molded article was further subjected to isostatic pressing at 200 MPa for 1 minute. This was put in an alumina crucible, spreaded with a powder, a compact was placed on it, covered, and the entire crucible was placed in a large carbon crucible. The temperature was raised to 1200 ° C.
  • ⁇ XRD measurement of sintered powder Part of the sintered body was pulverized using a magnetic mortar and pestle to obtain a powder. This powder was set in a glass holder and subjected to XRD measurement.
  • Example 2 (Production of sintered body containing YOF by pressure sintering) About 20 g of YOF powder (average particle diameter 0.8 ⁇ m) was placed in a rectangular mold having a length of 35 mm and a width of 35 mm, and primary molding was performed by a hydraulic press at a pressure of 18.4 MPa. This was put into a hot press die made of carbon having the same size as that of the square die and sintered by hot press. The temperature was raised to 1200 ° C. at 30 ° C./min in an Ar flow (flow rate 2 liters / minute), further raised to 1600 ° C. at 10 ° C./min, held at 1600 ° C. for 1 hour, and then 10 ° C./min.
  • Ar flow flow rate 2 liters / minute
  • the temperature was decreased to 1200 ° C., and then the temperature was decreased at 30 ° C./min. While being held at 1600 ° C. for 1 hour, uniaxial pressure was applied at a pressure of 36.7 MPa.
  • the three-point bending strength measured by the above method was 120 MPa.
  • the elastic modulus measured by the above method was 183 GPa, and the thermal conductivity measured by the above method was 17 W / (m ⁇ K).
  • the XRD of the obtained sintered powder was measured.
  • the obtained X-ray chart is shown in FIG. As shown in FIG.
  • Example 3 (Production of sintered body containing Y 5 O 4 F 7 by pressureless sintering) About 1.4 g of Y 5 O 4 F 7 powder (average particle size 1.1 ⁇ m) is placed in a circular mold having a diameter of 15 mm, uniaxially pressed with a hydraulic press at a pressure of 25.5 MPa, and held for 1 minute. Temporarily molded. The obtained temporary molded article was further subjected to isostatic pressing at 200 MPa for 1 minute. This was put in an alumina crucible, spreaded with a powder, a compact was placed on it, covered, and the entire crucible was placed in a large carbon crucible.
  • Example 4 (Production of sintered body containing Y 5 O 4 F 7 by pressure sintering). About 20 g of Y 5 O 4 F 7 powder (average particle diameter 1.1 ⁇ m) was placed in a rectangular mold having a length of 35 mm and a width of 35 mm, and was primary molded at a pressure of 18.4 MPa by a hydraulic press. This was put into a hot press die made of carbon having the same size as that of the square die and sintered by hot press. Under an Ar flow (flow rate 2 liters / minute), the temperature was raised to 1200 ° C. at 30 ° C./min, further raised to 1400 ° C. at 10 ° C./min, then lowered to 1200 ° C.
  • Ar flow flow rate 2 liters / minute
  • the XRD of the powder of the obtained sintered body was measured in the same manner as in Example 1.
  • the obtained X-ray chart is shown in FIG.
  • a peak considered to be derived from Y 5 O 4 F 7 is mainly observed, and very few peaks derived from components other than Y 5 O 4 F 7 are observed.
  • this sintered body is considered to contain 95% by mass or more of Y 5 O 4 F 7 .
  • Example 5 (Production of sintered body containing YOF by pressureless sintering)
  • the relative density RD is 87% and the open porosity is the same as in Example 1 except that the sintering is performed from the Ar atmosphere to the air atmosphere and the holding time at 1600 ° C. is changed from 1 hour to 2 hours.
  • a 0.2% sintered body was obtained.
  • this sintered body contained a large amount of Y 2 O 3 in addition to YOF.
  • CF 4 + O 2 plasma is irradiated to the surface of the sintered body obtained in Example 2, the single crystal of Comparative Example 1 and the sintered bodies of Comparative Examples 2 to 4 by a plasma processing apparatus (PT7160, Elminette). did. CF 4 was set to 0.8 scale, O 2 was set to 0.2 scale, and the output was 100 W and held for 30 minutes.
  • the solid surfaces of Example 2 and Comparative Examples 1 to 4 before and after plasma irradiation were observed with a scanning electron microscope (SEM). SEM photographs of the respective solid surfaces are shown in FIGS. 5 to 9, the upper side is an SEM photograph before irradiation, and the lower side is an SEM photograph after irradiation.
  • the yttrium oxyfluoride of Example 2 shows almost no change before and after irradiation.
  • the silicon of Comparative Example 1 was flat before irradiation, but it was confirmed that the surface was rough after irradiation.
  • the alumina which is Comparative Example 2 has a large number of white particles which were not seen before irradiation after irradiation.
  • the yttria which is the comparative example 3 does not change so much before and after irradiation.
  • the yttrium fluoride which is Comparative Example 4 has many cracks after irradiation.
  • the sintered body of yttrium oxyfluoride of Example 2 and the sintered body of yttria of Comparative Example 3 are more halogen-based than other sintered bodies and single crystals. It was shown to be resistant to plasma.
  • F / O atomic ratio before plasma irradiation F / O before irradiation
  • F / O atomic ratio after plasma irradiation F / O after irradiation
  • amount of change in F / O atomic ratio before and after plasma irradiation A graph showing (F / O after irradiation / F / O before irradiation) is shown in FIG.
  • ⁇ density
  • A is atomic weight
  • E 0 acceleration voltage
  • ⁇ 0 0.182
  • Z is an average atomic number.
  • the silicon (Si), alumina (Al 2 O 3 ), yttria (Y 2 O 3 ), and yttrium fluoride (YF 3 ) samples are irradiated with fluorine-based plasma.
  • the F / O ratio was greatly increased. That is, penetration of F element into the surface of these samples was observed.
  • the F / O ratio after irradiation is slightly less than twice before irradiation
  • Yttrium fluoride (YF 3 ) of Comparative Example 4 the F / O ratio after irradiation is low.
  • the upper left side is an SEM photograph
  • the upper right side is a fluorine atom distribution map
  • the lower right side is a platinum atom distribution map
  • the lower left side is a platinum atom distribution map and a fluorine atom distribution map.
  • the band-like one extending in the up-and-down direction is the platinum coat layer, and the left side is the sample.
  • the right side of the platinum layer is a redeposition layer during ion milling, and is not an original sample.
  • the left side of platinum is the surface of the sample.
  • the sintered body of the present invention is made of YOF, it originally contains elemental fluorine.
  • the gray portion other than the black portion corresponding to the platinum layer indicates the existence location of the fluorine atom, and this gray portion is from the black portion corresponding to platinum. Also spread across the left side.
  • fluorine is uniformly distributed regardless of the depth from the surface.
  • FIG. 12 in which a cross section of the sintered body after plasma irradiation is observed is gray in the fluorine atom distribution diagram on the upper right side. Since there is a part, fluorine exists in this part.
  • the existence site of fluorine atoms in the sintered body of Comparative Example 3 is platinum. Concentrated just to the left of the layer, which is about 50 nm from the sample surface. That is, it can be seen that in the yttria sintered body in Comparative Example 3, fluorine atoms entered the surface by plasma irradiation.
  • the sintered body of the present invention has higher corrosion resistance to the halogen-based plasma than any of the materials of Comparative Examples 1 to 4. Therefore, it is clear that the sintered body of the present invention is useful as a constituent member of a semiconductor manufacturing apparatus such as an etching apparatus.
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